WO2008149470A1 - Film de fines particules de fluor monocouche, corps stratifié à film de fines particules de fluor, ainsi que procédé de fabrication associé et dispositif d'affichage et photorécepteur et capteur, qui sont constitués à l'aide dudit film et dudit corps - Google Patents

Film de fines particules de fluor monocouche, corps stratifié à film de fines particules de fluor, ainsi que procédé de fabrication associé et dispositif d'affichage et photorécepteur et capteur, qui sont constitués à l'aide dudit film et dudit corps Download PDF

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Publication number
WO2008149470A1
WO2008149470A1 PCT/JP2007/061946 JP2007061946W WO2008149470A1 WO 2008149470 A1 WO2008149470 A1 WO 2008149470A1 JP 2007061946 W JP2007061946 W JP 2007061946W WO 2008149470 A1 WO2008149470 A1 WO 2008149470A1
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Prior art keywords
fluor
fine particle
film
base material
monolayer
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Application number
PCT/JP2007/061946
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English (en)
Inventor
Kazufumi Ogawa
Original Assignee
Kazufumi Ogawa
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Application filed by Kazufumi Ogawa filed Critical Kazufumi Ogawa
Priority to PCT/JP2007/061946 priority Critical patent/WO2008149470A1/fr
Publication of WO2008149470A1 publication Critical patent/WO2008149470A1/fr

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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/42Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00Coatings on glass
    • C03C2217/40Coatings comprising at least one inhomogeneous layer
    • C03C2217/42Coatings comprising at least one inhomogeneous layer consisting of particles only
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00Methods for coating glass
    • C03C2218/30Aspects of methods for coating glass not covered above
    • C03C2218/31Pre-treatment

Definitions

  • the present invention relates to a monolayer fluor fine particle film having even film thickness, a fluor fine particle film-layered body made by layering the monolayer fluor fine particle film, and a display device, photoreceptor, and sensor using them.
  • fluor fine particle includes mainly an alkali halide, rare earth ion fluor, manganese fluor, and sulfide fluor.
  • the fluor fine particle mentioned herewith includes so-called EL material.
  • LB Langmuir-Blodgett
  • CA chemical adsorption
  • a reference patent document includes, for example, Japanese Published Patent Application No. 2001-279471.
  • a covering film (hereafter, monolayer fluor fine particle film,) which is made by arranging only a monolayer of fluor fine particles on an arbitrary base material surface, having even thickness in a molecular size level, the covering film
  • fluor fine particle film-layered body made by layering a plurality of layers of the film, which is made by arranging fluor fine particles as only a monolayer, in a shape, and the manufacturing method thereof have not been yet developed and provided.
  • the present invention aims to provide, the covering film (monolayer fluor fine particle film,) which is made by arranging only a single layer of fluor fine particles on the arbitrary base material surface in the form, having even thickness in the molecular size level, the covering film (fluor fine particle film-layered body) made by layering the plurality of layers of the film, which is made by arranging fluor fine particles only as the monolayer, and the manufacturing method thereof.
  • the covering film monolayer fluor fine particle film, which is made by arranging only a single layer of fluor fine particles on the arbitrary base material surface in the form, having even thickness in the molecular size level
  • the covering film (fluor fine particle film-layered body) made by layering the plurality of layers of the film, which is made by arranging fluor fine particles only as the monolayer, and the manufacturing method thereof.
  • a first invention provided as a means for solving the problem is a monolayer fluor fine particle film having a covalent bond of a film of a monolayer of a fluor fine particle formed on a surface of a base material to a first organic film formed on the surface of the base material, through a second organic film formed on the surface of the fluor fine particle.
  • a second invention according to the first invention is the monolayer fluor fine particle film, wherein the first organic film formed on the surface of the base material and the second organic film formed on the surface of the fluor fine particle are different from each other.
  • a third invention according to the first invention is the monolayer fluor fine particle film, wherein the covalent bond is a -N-C- bond formed by a reaction of an epoxy group and an imino group.
  • a fourth invention according to the second invention is the monolayer fluor fine particle film, wherein the first organic film formed on the surface of the base material and the second organic film formed on the surface of the fluor fine particle are constituted of a monomolecular film.
  • a fifth invention according to the first to the fourth inventions is a display device, using the fluor fine particle film.
  • a sixth invention according to the first to the fourth inventions is a photoreceptor, using the fluor fine particle film.
  • a seventh invention according to the first to the fourth invention is a sensor, using the fluor fine particle film.
  • An eighth invention is a manufacturing method for the monolayer fluor fine particle film, comprising: a step of forming a first reactive organic film on the surface of the base material by contacting the surface of the base material with a chemical adsorption solution prepared by blending at least a first alkoxysilane compound and a silanol condensation catalyst and a nonaqueous organic solvent to react an alkoxysilane compound to the surface of the base material; a step of forming a second reactive organic film on the surface of the fluor fine particle by dispersing the fluor fine particle in chemical adsorption solution prepared by blending at least a second alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the fluor fine particle; a step of contacting, for a reaction, the fluor fine particle covered with the second reactive organic film to the surface of the
  • a ninth invention according to eighth invention is the manufacturing method for the monolayer fluor fine particle film, comprising: the step of forming the first reactive organic film on the surface of the base material by contacting the surface of the base material with the chemical adsorption solution prepared by blending at least the first alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react an alkoxysilane compound to the surface of the base material and a step of forming the second reactive organic film on the surface of the fluor fine particle by dispersing the fluor fine particle in chemical adsorption solution prepared by blending at least the second alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the fluor fine particle, followed by washing each of the base material and the surface of the fluor fine particle with an organic solvent to form a first and second reactive monomolecular films having the covalent bond to the base material and the surface of the fluor fine particle.
  • a tenth invention according to eighth invention is the manufacturing method for the monolayer fluor fine particle film, wherein the first reactive organic film contains an epoxy group and the second reactive organic film contains an imino group or the first reactive organic film contains the imino group and the second reactive organic film contains the epoxy group.
  • An eleventh invention according to ninth invention is the manufacturing method for the monolayer fluor fine particle film, wherein the first reactive monomolecular film contains an epoxy group and the second reactive monomolecular film contains an imino group or the first reactive monomolecular film contains the imino group and the second reactive monomolecular film contains the epoxy group.
  • a twelfth invention is a fluor fine particle film-layered body wherein the fluor fine particle layered as stratification on the surface of the base material has the covalent bond between layers through an organic covering film formed on the surface of the fluor fine particle.
  • a thirteenth invention according to twelfth invention is the fluor fine particle film-layered body, wherein there are 2 kinds of organic covering films formed on the surface of the fluor fine particle, the fluor fine particle, on which the first organic film is formed, and the fluor fine particle, on which the second organic film is formed, are layered alternately.
  • a fourteenth invention according to thirteenth invention is the fluor fine particle film-layered body, wherein the first organic film reacts to the second organic film to form the covalent bond.
  • a fifteenth invention according to twelfth invention is the fluor fine particle film-layered body, wherein the covalent bond is the -N-C- bond formed by the reaction of the epoxy group to the imino group.
  • a sixteenth invention is the display device, using the fluor fine particle film-layered body according to the twelfth to the fifthteenth inventions.
  • a seventeenth invention is a photoreceptor, using the fluor fine particle film-layered body according to twelfth to fifthteenth inventions.
  • An eighteenth invention is a sensor, using the fluor fine particle film-layered body according to twelfth to fifthteenth inventions.
  • a nineteenth invention is a manufacturing method for the fluor fine particle film-layered body using: the step of forming the first reactive organic film on the surface of the base material by contacting the surface of the base material with the chemical adsorption solution prepared by blending at least the first alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the base material; the step of forming the second reactive organic film on the surface of the first fluor fine particle by dispersing the first fluor fine particle in chemical adsorption solution prepared by blending at least the second alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the fluor fine particle; the step of contacting, for the reaction, the first fluor fine particle covered with the second reactive organic film to the surface of the base material having the first reactive organic film formed thereon; the step of washing out the first fluor fine particle covered with the excessive second reactive organic film to form the first
  • a twenty first invention according to nineteenth invention is the manufacturing method for the fluor fine particle film-layered body of a multilayer structure, wherein, following the step of forming the second monolayer fluor fine particle film, similarly, the step of forming the first monolayer fluor fine particle film and the step of forming the second monolayer fluor fine particle film are repeated.
  • a twenty second invention according to nineteenth invention is the manufacturing method for the fluor fine particle film-layered body, wherein, following the step of forming the first to third reactive organic films, for each of their steps, surfaces of the base material or the fluor fine particle are washed with the organic solvent to form the first to third reactive monomolecular films having the covalent bond to the surface of the base material and the fluor fine particle.
  • a twenty third invention according to nineteenth invention is the manufacturing method for the fluor fine particle film-layered body, wherein the first and third reactive organic films contain the epoxy group and the second reactive organic film contains the imino group or the first and third reactive organic films contain the imino group and the second reactive organic film contains the epoxy group.
  • a twenty fourth invention according to the fifth and the nineteenth inventions is the manufacturing method for the monolayer fluor fine particle film and the fluor fine particle film-layered body, wherein, replacing to the silanol condensation catalyst, a ketimine compound or an organic acid, aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound are used.
  • a twenty fifth invention according to fifth and nineteenth inventions is the manufacturing method for the fluor fine particle film-layered body, wherein the silanol condensation catalyst is blended with ketimine compound or at least 1 selected from an organic acid, aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound for use as a promoter.
  • the present invention aims to provide the monolayer fluor fine particle film, wherein the monolayer film of the fluor fine particle, which is formed on the surface of the base material, has the mutual covalent bond to the first organic film, which is formed on the surface of the base material, through the second organic film formed on the surface of the fluor fine particle, by: a step of forming a first reactive organic film on the surface of the base material by contacting the surface of the base material with a chemical adsorption solution prepared by blending at least a first alkoxysilane compound and a silanol condensation catalyst and a nonaqueous organic solvent to react an alkoxysilane compound to the surface of the base material; a step of forming a second reactive organic film on the surface of the fluor fine particle by dispersing the fluor fine particle in chemical adsorption solution prepared by blending at least a second alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the
  • Containing the epoxy group in the first reactive organic film and containing the imino group in the second reactive organic film or containing the imino group in the first reactive organic film and containing the epoxy group in the second reactive organic film is preferable for preparing the monomolecular fluor fine particle film having the covalent bond on the surface of the base material.
  • Containing an epoxy group in the first reactive monomolecular film and containing an imino group in the second reactive monomolecular film or containing the imino group in the first reactive monomolecular film and containing the epoxy group in the second reactive monomolecular film is preferable for preparing the monomolecular fluor fine particle film having the covalent bond on the surface of the base material.
  • ketimine compound or the organic acid, aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound is preferable for shortening the time for fabricating the film.
  • ketimine compound or at least 1 selected from the organic acid, aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound is preferable for shortening further the time for fabricating the film.
  • Making different the first organic film, which is formed on the surface of the fluor fine particle, from the second organic film formed on the surface of the base material, is preferable for binding a single layer of the monolayer fluor fine particle film on the surface of the base material.
  • the covalent bond is preferable for providing the monolayer fluor fine particle film excellent in adhesion strength against the base material.
  • the present invention provides the fluor fine particle film-layered body having the covalent bond of fluor fine particles, which is made by layering on the surface of the base material in stratification, between each other layer through the organic film, which is formed on the surface of the fluor fine particle, by: the step of forming the first reactive organic film on the surface of the base material by contacting at least the surface of the base material with the chemical adsorption solution prepared by blending the first alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the base material; the step of forming the second reactive organic film on the surface of the first fluor fine particle by dispersing the first fluor fine particle in chemical adsorption solution prepared by blending at least the second alkoxysilane compound
  • the fluor fine particle film-layered body having the multilayer structure can be readily manufactured.
  • washing the surface of the base material or the fluor fine particle with the organic solvent to form the first to third reactive monomolecular films having the covalent bond to the surfaces of the base material and the fluor fine particle is preferable for making the film thickness of the fluor fine particle film-layered body even.
  • Containing the epoxy group in the first and third reactive organic films and containing the imino group in the second reactive organic film or containing the imino group in the first and third reactive organic films and containing the epoxy group in the second reactive organic film are preferable for manufacturing the fluor fine particle film-layered body the covalent bond between layers by the reaction of the epoxy group to the imino group.
  • silanol condensation catalyst Using by blending the silanol condensation catalyst with ketimine compound or at least 1 selected from the organic acid, aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound as the promoter is preferable for further shorten the time for making the film.
  • the covalent bond made by reaction of the first organic film and the second organic film is preferable for providing the fluor fine particle film-layered body excellent in adhesion strength.
  • using the -N-C- bond, which is formed by the reaction of the epoxy group to the imino group, as the covalent bond is preferable for providing the fluor fine particle film-layered body excellent in strength.
  • the covering film (monolayer fluor fine particle film) made by the arrangement of only 1 layer of the fluor fine particles on the surface of the arbitrary base material and having the even thickness in the particle size level; the covering film (fluor fine particle film-layered body) made by layering the plurality of films made by arranging only 1 layer of the fluor fine particles; and manufacturing methods for them at a low cost.
  • FIG. 1 is a conceptual rendering obtained by molecular level enlargement of the reaction of the surface of the fluor fine particle in the first example according to the present invention
  • FIG. 1A is a figure of the surface of the zinc sulfate fluor fine particle before the reaction
  • FIG. 1 B is the figure after the monomolecular film containing the epoxy group was formed
  • FIG. 1 C is the figure after the monomolecular film containing the amino group was formed.
  • FIG. 2 is the conceptual rendering obtained by molecular level enlargement of the reaction of the surface of the glass base material in the second example according to the present invention
  • FIG. 2A is the figure of the surface before the reaction
  • FIG. 2B is the figure after the monomolecular film containing the epoxy group was formed
  • FIG. 2C is the figure after the monomolecular film containing the amino group was formed.
  • FIG. 3 is the conceptual rendering made by molecular level enlargement of the reaction of the surface of the glass base material in the third and fourth examples according to the present invention
  • FIG. 3A shows the figure of the surface of the base material, on which the monolayer zinc sulfate fluor fine particle film is formed
  • FIG. 3B shows the figure of the surface of the base material, on which two layers of the monolayer zinc sulfate fluor fine particle film were formed.
  • the present invention provides a display device, photoreceptor, and sensor using the fluor fine particle film-layered body having the covalent bond of fluor fine particles, which is made by layering on the surface of the base material in stratification, between each other layer through the organic film, which is formed on the surface of the fluor fine particle, by: the step of forming the first reactive organic film on the surface of the base material by contacting at least the surface of the base material with the chemical adsorption solution prepared by blending the first alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the base material; the step of forming the second reactive organic film on the surface of the first fluor fine particle by dispersing the first fluor fine particle in chemical adsorption solution prepared by blending at least the second alkoxysilane compound and the silanol condensation catalyst and the nonaqueous organic solvent to react the alkoxysilane compound to the surface of the fluor fine particle; the step of contacting
  • the present invention has the effect of providing a product by using the covering film (monolayer fluor fine particle film) made by the arrangement of only 1 layer of the fluor fine particles on the surface of the arbitrary base material and having the even thickness in the particle size level and the covering film (fluor fine particle film-layered body) made by layering the plurality of films made by arranging only 1 layer of the fluor fine particles, and a manufacturing method for them conveniently at a low cost.
  • the covering film monolayer fluor fine particle film
  • the covering film fluor fine particle film-layered body
  • the fluor fine particle of the monolayer fluor fine particle film and the fluor fine particle film-layered body according to the present invention includes mainly an alkali halide, rare earth ion fluor, manganese fluor, and sulfide fluor.
  • a zinc sulfate fine particle fluor will be described below as the typical example.
  • an anhydrous zinc sulfate fine particle 1 having a size of about 100 nm was prepared and dried well.
  • the reactive functional group such as the epoxy group or the imino group as the chemical adsorbent in the functional site and the drug containing the alkoxy silyl group, which is exemplified by the drug shown by the following formula (chemical formula C1 ) or (chemical formula C2,) in the other terminal were weighed to make 99 weight percent each, and, dibutyltin diacetylacetonate or acetic acid being an organic acid, for example, as a silanol condensation catalyst is weighed to make about 1 weight percent.
  • Anhydrous zinc sulfate fluor fine particle 1 was mixed with this adsorbent solution, stirred, and reacted in normal air (relative humidity 45%) for about 2 hours. At this time, a dangling bond of the surface of the anhydrous zinc sulfate fluor fine particle contains many hydroxyl groups 2 (FIG.
  • the tin-based catalyst causes a precipitation and, therefore, the organic acid such as the acetic acid should be used.
  • the amino group contains the imino group.
  • Substances, except the amino group, containing the imino group include a pyrrole derivative and imidazol derivative.
  • using a ketimine derivative allows introducing easily the amino group by hydrolysis following formation of the covering film.
  • This covering film has the film thickness very thin on the nanometer level and, therefore, showed no loss of the particle size.
  • glass base material 11 was prepared and dried well.
  • the reactive functional group such as the epoxy group or the imino group as the chemical adsorbent in the functional site and the drug containing the alkoxy silyl group, which is exemplified by the drug shown by the formula (chemical formula C1 ) or (chemical formula C2,) as described above in the other terminal were weighed to make 99 weight percent each, and, dibutyltin diacetylacetonate, for example, as the silanol condensation catalyst is weighed to make about 1 weight percent.
  • All these drugs were dissolved in the silicon solvent, for example, the hexamethyl disiloxane solvent to make about 1 weight percent concentration (preferable concentration of the chemical adsorbent ranges from about 0.5 to 3%) to prepare the chemical adsorbent solution.
  • glass base material 11 was soaked in this adsorbent solution for reaction in normal air (relative humidity 45%) for about 2 hours.
  • the surface of glass base material 11 contains many hydroxyl groups 12 (FIG. 2A) and, thus, -Si- (OCH 3 ) group of the chemical adsorbent causes dealcohol (in this case, deCHaOH) reaction to the hydroxyl groups in the presence of the silanol condensation catalyst to make the bond shown in the formula (chemical formula C3) or (chemical formula C4) resulting in the formation of the chemical adsorption monomolecular film 13 (FIG. 2B 1 ) which contains the epoxy group chemically bonded to the surface across all the surface of glass base material 11 , (or the chemical adsorption film 14 containing the amino group (FIG. 2C) in the film thickness of about 1 nanometer.
  • This covering film has the film thickness very thin on the nanometer level and, therefore, showed no loss of the clarity of the glass base material.
  • replacement is a combination of the zinc sulfate fluor fine particle covered with the chemical adsorption monomolecular film having the epoxy group and the surface of the glass base material covered with the chemical adsorption monomolecular film having the amino group
  • alcohol to be applied and heated in this example, 100 deg C.
  • the amino group on the surface of the zinc sulfate fluor fine particle contacting to the epoxy group on the surface of the glass base material was added by the reaction shown by the following formula (Chemical formula C5) to bind the fluor fine particle to the glass base material through the two monomolecular films resulting in the final hardening.
  • evaporating alcohol irradiating an ultrasonic wave enabled to improve the evenness of the film thickness of the covering film.
  • the covering film of the zinc sulfate fluor fine particle which is covered with the chemical adsorption monomolecular film having the epoxy group
  • the monolayer fluor fine particle film was formed in the state of only single layer arrangement of the zinc sulfate fluor fine particles covered with the chemical adsorption monomolecular film having the epoxy group with the covalent bond to the surface of glass base material, having the even thickness in the particle size level.
  • the thickness of the monolayer fluor fine particle film of the zinc sulfate fluor fine particles was about 100 nm with very even thickness and, hence, interference colors were never observed.
  • Example 4 when thickening the film thickness of the fluor fine particle film is desired, following Example 3, zinc sulfate fluor fine particle 5 covered with the chemical adsorption monomolecular film having the epoxy group was dispersed in alcohol, applied to the surface of glass base material 15, on which the monolayer fluor fine particle film 17 was formed in the state of only single layer arrangement of the zinc sulfate fluor fine particles covered with the chemical adsorption monomolecular film having the amino group with the covalent bond, having the even thickness on the particle size, and heated (in the present example, to 100 deg C.) Then, the epoxy group on the surface of the zinc sulfate fluor fine particle contacting to the amino group on the surface of the glass base material, on which the monolayer fluor fine particle film of the zinc sulfate fluor fine particle covered with the chemical adsorption monomolecular film having the amino group was formed, was added by the reaction shown by the formula (Chemical formula C5) to bind the zinc sulf
  • (CH 2 OCH)- group represents the functional group expressed by the following formula (Chemical formula C7) and (CH 2 CHOCH (CH 2 ) 2 ) CH- group represents the functional group expressed by the following formula (Chemical formula C8.) [C6] O CH 2 -CH
  • usable silanol condensation catalysts include a metal salt of a carboxylic acid, the metal salt of a carboxylic acid ester, polymer of the metal salt of the carboxylic acid, a chelate of the metal salt of the carboxylic acid, titanic acid ester, and chelates of the titanic acid ester.
  • Usable solvents for a film formation solution were an organic chlorine-based solvent containing no water, hydrocarbon-based solvent, or carbon fluoride-based solvent, and silicone-based solvent, or a mixture thereof.
  • a boiling point of the solvent ranges preferably from about 50 to 250 deg C.
  • alcohol-based solvents such as methanol, ethanol, and propanol or the mixture thereof could be used.
  • Specifically usable solvents include a chlorosilane-based nonaqueous petroleum naphtha, solvent naphtha, petroleum ether, petroleum benzene, isoparaffin, normal paraffin, decalin, industrial gasoline, nonane, decane, kerosine, dimethyl silicone, phenyl silicone, alkyl denatured silicone, polyether silicone, and dimethyl formamide.
  • Carbon fluoride-based solvents include freon-based solvent, Frorinate (made by Sumitomo 3M Limited,) and Aflude (Asahi Glass Co. made.) These may be singly used as the monolayer and, if they are blended well, may be used in a combination of two kinds.
  • the organic chlorine-based solvent such as chloroform may be added.
  • silanol condensation catalysts as described above were replaced for use by the ketimine compound or the organic acid, the aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound, a process time could be shorten to make a half to 2/ 3 of the time necessary for the same concentration.
  • silanol condensation catalyst by mixing (a range from 1 :
  • 9 to 9: 1 can be applied, but normally around 1 : 1 is preferable) with the ketimine compound or the organic acid, the aldimine compound, enamine compound, oxazolidine compound, and aminoalkyl alkoxy silane compound can make the process time fast several-fold (up to about 30 minutes) resulting in shortening of the time for making the film up to several-fold decrease.
  • dibutyltin oxide being the silanol catalyst was replaced by Japan Epoxy Resin Co. made H3 being the ketimine compound under the same condition. Almost same result was obtained except that the reaction time became short to about 1 hour.
  • the silanol catalyst was replaced by the mixture (mixture ratio was
  • usable ketimine compounds are not specially restricted, but include, for example, 2,5,8-triaza-1 ,8-nonadiene,
  • Usable organic acids are not specially restricted, but include, for example, formic acid, or acetic acid, propionic acid, butyric acid, and malonic acid and showed the almost same effect.
  • the monolayer fluor fine particle film and the fluor fine particle film-layered body enables to manufacture the display device excellent in evenness of brightness, photoreceptor excellent in evenness of display quality, and sensor excellent in evenness of sensitivity.
  • the description is made for the zinc sulfate fluor fine particle and the glass base material as examples of the fluor.
  • the present invention can be applied to the alkali halide, rare earth ion fluor, manganese fluor, and sulfide fluor, and also applied to an organic fluor of which surface has an active hydrogen such as the hydroxyl group and the imino group.
  • application of the present invention includes a display, fluorescent lighting, indication board, photographic plate, for example, for an X-ray, optical recording medium, electronic photographic image bar, and gas concentration sensor.

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Abstract

De fines particules de fluor de taille micrométrique ou de taille nanométrique ont été développées et fabriquées. Une utilisation efficace des fonctions inhérentes desdites fines particules de fluor nécessite la préparation de fines particules de fluor dans un film de couverture présentant une épaisseur uniforme. Cependant, on a jamais eu l'idée de fabriquer un film de couverture d'épaisseur uniforme au niveau de la taille des particules à l'aide desdites fines particules de fluor. Un film de fines particules de fluor monocouche, présentant une liaison covalente d'un film d'une monocouche de fines particules de fluor, qui est formé sur une surface d'un matériau de base, sur un premier film organique formé sur la surface du matériau de base, à travers un second film organique formé sur la surface de la fine particule de fluor. Le premier film de couverture organique formé sur la surface du matériau de base diffère du second film organique formé sur la surface de la fine particule de fluor.
PCT/JP2007/061946 2007-06-07 2007-06-07 Film de fines particules de fluor monocouche, corps stratifié à film de fines particules de fluor, ainsi que procédé de fabrication associé et dispositif d'affichage et photorécepteur et capteur, qui sont constitués à l'aide dudit film et dudit corps WO2008149470A1 (fr)

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PCT/JP2007/061946 WO2008149470A1 (fr) 2007-06-07 2007-06-07 Film de fines particules de fluor monocouche, corps stratifié à film de fines particules de fluor, ainsi que procédé de fabrication associé et dispositif d'affichage et photorécepteur et capteur, qui sont constitués à l'aide dudit film et dudit corps

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PCT/JP2007/061946 WO2008149470A1 (fr) 2007-06-07 2007-06-07 Film de fines particules de fluor monocouche, corps stratifié à film de fines particules de fluor, ainsi que procédé de fabrication associé et dispositif d'affichage et photorécepteur et capteur, qui sont constitués à l'aide dudit film et dudit corps

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003168606A (ja) * 2001-01-24 2003-06-13 Matsushita Electric Ind Co Ltd 微粒子配列体とその製造方法及びこれを用いたデバイス
JP2007118276A (ja) * 2005-10-26 2007-05-17 Kagawa Univ 単層微粒子膜と累積微粒子膜およびそれらの製造方法。
JP2007127847A (ja) * 2005-11-04 2007-05-24 Kagawa Univ 反射防止膜とその製造方法及びそれを用いた光学機器

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003168606A (ja) * 2001-01-24 2003-06-13 Matsushita Electric Ind Co Ltd 微粒子配列体とその製造方法及びこれを用いたデバイス
JP2007118276A (ja) * 2005-10-26 2007-05-17 Kagawa Univ 単層微粒子膜と累積微粒子膜およびそれらの製造方法。
JP2007127847A (ja) * 2005-11-04 2007-05-24 Kagawa Univ 反射防止膜とその製造方法及びそれを用いた光学機器

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